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作 者:王巨存[1] 谢宪斌[2] 冯鑫[1] 赵薇[1] 郑榕[1] 房德敏[1] 李燕[3]
机构地区:[1]天津市天津医院药学部,天津300211 [2]天津医科大学药学院,天津300070 [3]天津市天津医院骨科研究所,天津300211
出 处:《药物分析杂志》2014年第3期418-422,共5页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:采用HPLC法同时测定壮骨止痛颗粒(淫羊藿、蛇床子、延胡索)中的淫羊藿苷、延胡索乙素和蛇床子素的含量。方法:采用SymmetryC18(150mm×3.9mm,5μm)色谱柱,以乙腈(A)-0.1%磷酸溶液(B;三乙胺调pH至6.5)为流动相,梯度洗脱(0~24min,24.5%A;24—70min,24.5%A-57.5%A),流速0.8mL·min^-1,柱温35℃,检测波长270nm(0~25min)、282nm(25-55min)、322nm(55~70min),进样量20μL。结果:淫羊藿苷、延胡索乙素和蛇床子素的线性范围分别为0.255.0.561mg·mL^-1(r=0.9996)、6.40~14.08μg·mL^-1(r=0.9998)、0.170—0.510mg·mL^-1(r=0.9999);—平均加样回收率(n=6)分别为99.19%(RSD=1.2%)、99.97%(RSD=0.89%)、99.71%(RSD=1.2%)。结论:本方法方法学验证可用于壮骨止痛颗粒的质量控制。Objective: To simultaneously determine the contents of icariin, tetrahydropalmatine and osthole in Zhuanggu Zhitong granules. Methods: RP - HPLC method was used. The determination was performed on a Sym- metry C18 column (150 mm x3.9 mm,5 μm)with mobile phase consisting of acetonitrile(A) -0. 1% phosphoric acid ( B ; adjusted pH to 6.5 with triethylamine) in gradient elution (0 - 24 min,24. 5 % A ; 24 - 70 min, 24. 5 % A→57.5% A). The flow rate was 0. 8 mL · min-1. The column temperature was 35 ℃. The detection wavelength was set at 270 nm in 0 - 25 min,282 nm in 25 - 55 min, and 322 nm in 55 - 70 rain. Injection volume was 20 μL. Results: The linear ranges of icariin, tetrahydropalmatine and osthole were 0. 255 - 0. 561 mg · mL-1 ( r = 0. 9996) ,6. 40 - 14.08 μg · mL-1 ( r = 0. 9998) and 0. 170 - 0. 510 mg · mL-1 ( r = 0. 9999 ), respectively. The average recoveries(n =6) were 99. 19% (RSD = 1.2%),99.97% (RSD =0.89%) and 99.71% (RSD = 1.2% ) , respectively. Conclusion: The method can be used for the quality control of Zhuanggu Zhitong granules by methodology validation.
关 键 词:反相高效液相色谱法 淫羊藿苷 延胡索乙素 蛇床子素 壮骨止痛颗粒 中成药质量控制 方法验证
分 类 号:R917[医药卫生—药物分析学]
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